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Journal of Environmental Protection, 2012, 3, 107-113

http://dx.doi.org/10.4236/jep.2012.31013 Published Online January 2012 (http://www.SciRP.org/journal/jep)

13

Biodiesel Production from Waste Cooking Oil Using


Sulfuric Acid and Microwave Irradiation Processes
Prafulla D. Patil, Veera Gnaneswar Gude, Harvind K. Reddy, Tapaswy Muppaneni, Shuguang Deng*
Chemical Engineering Department, New Mexico State University, Las Cruces, USA.
Email: *sdeng@nmsu.edu
Received July 30th, 2011; revised October 1st, 2011; accepted November 15th, 2011

ABSTRACT
A comparative study of biodiesel production from waste cooking oil using sulfuric acid (Two-step) and microwaveassisted transesterification (One-step) was carried out. A two-step transesterification process was used to produce biodiesel (alkyl ester) from high free fatty acid (FFA) waste cooking oil. Microwave-assisted catalytic transesterification
using BaO and KOH was evaluated for the efficacy of microwave irradiation in biodiesel production from waste cooking oil. On the basis of energy consumptions for waste cooking oil (WCO) transesterification by both conventional
heating and microwave-heating methods evaluated in this study, it was estimated that the microwave-heating method
consumes less than 10% of the energy to achieve the same yield as the conventional heating method for given experimental conditions. The thermal stability of waste cooking oil and biodiesel was assessed by thermogravimetric analysis
(TGA). The analysis of different oil properties, fuel properties and process parametric evaluative studies of waste cooking oil are presented in detail. The fuel properties of biodiesel produced were compared with American Society for
Testing and Materials (ASTM) standards for biodiesel and regular diesel.
Keywords: Biodiesel; Waste Cooking Oil; Free Fatty Acid; Sulfuric Acid; Microwave-Assisted Transesterification

1. Introduction
The current methods to produce, convert and consume
energy derived from fossil fuels throughout the world are
not sustainable. Due to limited amounts of fossil fuels
and increasing concerns of global warming, there is evergrowing urge to develop fuel substitutes that are renewable and sustainable. Biomass derived fuels such as methane, ethanol, and biodiesel are well-accepted alternatives to diesel fuels as they are economically feasible,
renewable, environmental-friendly and can be produced
easily in rural areas where there is an acute need for modern forms of energy.
Edible vegetable oils such as canola, soybean, and corn
have been used for biodiesel production and are proven
diesel substitutes [1,2]. However, a major obstacle in the
commercialization of biodiesel production from edible
vegetable oils is their high production cost, which is due
to the demand for human consumption. Reducing the
cost of the feedstock is necessary for biodiesels longterm commercial viability. One way to reduce the cost of
this fuel is to use less expensive feedstocks including
waste cooking oils and vegetable oils that are non-edible
and/or require low harvesting costs. Waste cooking oil
*

Corresponding author.

Copyright 2012 SciRes.

(WCO), which is much less expensive than edible vegetable oil, is a promising alternative to edible vegetable oil
[3]. Waste cooking oil and fats set forth significant disposal problems in many parts of the world. This environmentally-threatening problem could be turned into
both economical and environmental benefit by proper
utilization and management of waste cooking oil as a fuel
substitute. Many developed countries have set policies
that penalize the disposal of waste cooking oil into waste
drainage [4]. The Energy Information Administration
(EIA) in the United States (USA) estimated that around
100 million gallons of waste cooking oil is produced per
day in USA, where about 9 pounds of waste cooking oil
are generated per person per year [5]. The estimated
amount of waste cooking oil collected in Europe is about
0.49 - 0.7 million gallons/day [6]. Waste cooking oil, as
an alternative feedstock for biodiesel, was studied with
different aspects such as optimization using supercritical
methanol (SCM) transesterification, process design and
technological assessment, fuel property analysis and cost
estimation approaches [7-9].
Biodiesel is derived from fats and oils either by
chemical or bio-chemical means [10]. There are at least
four ways in which oils and fats can be converted into
biodiesel, namely, transesterification, blending, microJEP

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Biodiesel Production from Waste Cooking Oil Using Sulfuric Acid and Microwave Irradiation Processes

emulsions and pyrolysis. Among these, transesterification is the most commonly used method as it reduces the
viscosity of oil [11]. Biodiesel production by transesterification reaction can be catalyzed with alkali, acidic or
enzymatic catalysts. Alkali and acid transesterification
processes require less reaction time with reduced processing costs as compared to the enzyme catalyst process
[12,13]. Alkali process yields high quantity and high
purity biodiesel in shorter reaction time [14]; however,
this process is not suitable for feedstock with high free
fatty acid (FFA) content. Therefore, a two-step transesterification process (acid esterification followed by
alkali transesterification) was developed to remove high
free fatty acid (FFA) content and to improve the biodiesel yield. The long reaction time and low recovery of
catalyst were disadvantages of the two-step process. An
alternative method, namely the microwave-assisted catalytic transesterification, has been developed that gives high
biodiesel yield and purity. Microwave-assisted transesterification is an energy-efficient and a quick process
to produce biodiesel from different feedstocks [15,16].
Microwave-heating has been successfully applied to
synthesize porous materials and supported catalyst in our
previous research [17,18]. Microwave-assisted transesterification of different feedstocks such as rapeseed oil,
cotton seed oil and waste cooking oils has been reported
by several researchers [15,19,20].
In this research, we have conducted several experiments to compare the biodiesel production from waste
cooking oil using sulfuric acid (Two-step) and microwave-assisted transesterification (One-step) processes.
Since waste cooking oil contains high FFA content, a
two-step process, acid esterification followed by alkali
transesterification was employed using methanol, sulfuric acid and KOH catalyst. Microwave-assisted catalytic
transesterification using BaO and KOH was studied for
waste cooking oil to compare with the conventional
heating method. Energy requirements for both conventional and microwave heating methods and product separation times were compared.

2. Methodology
Waste cooking oil (WCO) was collected from a local
restaurant in Las Cruces, NM. Potassium hydroxide
flakes, methanol (AR Grade), and diethyl ether were
procured from Fisher Scientific, New Jersey. Sulfuric
acid (98% pure) was procured from Acros Organics,
New Jersey. The mixture was stirred at the same speed
for all test runs. All experiments of transesterification
reaction were performed in a 250 mL round-bottom flask
equipped with a water-cooled reflux condenser. A hot
plate with magnetic stirrer arrangement was used for
heating the mixture in the flask. The microwave-assisted
transesterification was performed using a modified doCopyright 2012 SciRes.

mestic microwave oven (with an output power of 800 W).


The microwave oven was modified and fitted with a
temperature reader, an external agitator and a watercooled reflux condenser.

2.1. Characteristics of Waste Cooking Oil


The quality of oil is expressed in terms of the physicochemical properties such as acid value, saponification
value, and iodine value. The saponification value of
waste cooking oil (WCO) was reported as 186.3 (mg
KOH/g). The acid value of waste cooking oil was found
to be 17.41 mg KOH/gm. It has been reported that transesterification would not occur if FFA content in the oil
were above 3 wt% [21].

2.2. Transesterification Reaction


The transesterification process was widely used in biodiesel production from different biomass materials. The
process consists of two steps namely, acid esterification
and alkali transesterification [22]: Step 1: Acid esterification: Acid esterification reduces the FFA value of unrefined oil using an acid catalyst. Step 2: Alkali transesterification: After removing the impurities of the product from the Step 1, it is transesterified to monoesters of
fatty acids using an alkali catalyst.
The mechanism of synthesis of biodiesel via two-step
transesterification process is represented as
Acid Esterification (Step 1)
RCOOH + CH3OH

H2SO4

RCOOH3 + H2O

Acid Transesterification (Step 2)


CH2OOCR1

CHOOCR2

R1COOH3

+ 3CH3OH

KOH

Triglyceride

R2COOH3 + CHOH

R3COOH3

CH2OOCR3
Methanol

CH2OH

CH2OH

Methyl Ester Glycerol

For microwave transesterification procedure, the calculated amount of waste cooking oil was added to the
premixed solution of methanol and catalysts (KOH and
BaO). The mixture was then subjected to the microwave
irradiation with exiting power of 800 W, under a matrix
of conditions: methanol to oil molar ratio of 6:1 to 15:1;
catalyst concentrations in the range 1 - 2 wt% of oil with
constant reaction time of 6 min. The purification and
separation steps (downstream procedure) are described
elsewhere [23].

2.3. Analysis of Biodiesel


For the quantification of reaction products, the samples
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Biodiesel Production from Waste Cooking Oil Using Sulfuric Acid and Microwave Irradiation Processes

A AEI CEI VEI 100%


AEI

The biodiesel yield is apparently same to that of the


FAME Content (%) calculated quantitatively by GC-MS
[24]. Where A total peak area of methyl ester, AEI
peak area of methyl heptadeconoate, CEIconcentration
(mg/mL) of standard solution (methyl heptadecanoate),
VEIvolume (mL) of standard solution (methyl heptadecanoate) and Wweight (mg) of sample. From GCMS and TIC analysis, it can be noted that waste cooking
biodiesel contains major proportion of unsaturated fatty
acids.

excess methanol in the ester layer can be removed by


distillation. Canakci and Van Gerpan [25] advocate the
use of large excess quantities of methanol (15:1-35:1)
while using the sulphuric acid as catalyst. Figure 2
shows the methanol to oil molar ratio effect in alkali
transesterification (Step 2). At higher levels, an excess
methanol amount may reduce the concentration of the
catalyst in the reactant mixture and retard the transesterification reaction [26].
An alkali catalyst was studied in the range of 0.3% to
2.5% using KOH as an alkali catalyst. The influence of
the alkali catalyst amount on the yield is shown in Figure 3. The maximum yield was achieved for waste
cooking oil at 2% of catalyst loading. During the experiments, it was also observed that transesterification could
not take place properly with an insufficient amount of an
alkali catalyst loading. The production yield slightly decreased above 2% of catalyst loading. At higher concentrations, the intensification of mass transfer became more
important than increasing the amount of catalyst. The
reaction temperature effect on the yield was studied in
the temperature range of 40C to 100C at atmospheric
100

90

Biodiesel Yield (%)

were analyzed by a gas chromatography-mass spectrometry (GC-MS) system incorporated with an Agilent
5975 C mass-selective detector (MSD) and an Agilent
7890 A gas chromatograph equipped with a capillary
column (HP-5 MS, 5% phenyl methyl silox 30 m 250
m 0.25 m nominal). Methyl heptadecanoate (10.00
mg; internal standard) was dissolved in 1 mL heptane to
prepare the standard solution. Approximately 55 mg
methyl ester was dissolved in 1 mL standard solution for
GC analysis. Approximately 1 L sample was injected
into the GC. Helium was used as the carrier gas. The
injection was performed in splitless mode. The parameters of the oven temperature program consist of: start at
80C with 10C/min intervals up to 180C (1 min) and up
to 255C with 15C/min intervals (2 min). The Fatty acid
methyl ester (FAME) content was calculated by use of
the equation:

3. Results and Discussion

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70

60

50

3.1. Sulfuric Acid Process


(Two-Step Transesterification)

40
0

0.5

1.5

2.5

Acid Conc.( v/v %)

Figure 1. Effect of acid concentration on biodiesel yield


(Step 1) in sulfuric acid process.
100

B iodiesel Y ield (% )

Acid esterification reaction was studied for four different


molar ratios. The sulfuric acid catalyst amount was varied in the range of 0.3% to 2%. These percentages are
based on volume of the oil used for the acid esterification
reaction. The catalyst amount also affects the yield of
process is shown in Figure 1. The acid-catalyst process
attained maximum yield for waste cooking oil at 0.5%
catalyst concentration. It was observed that the yield
started to decline when the catalyst concentration was
increased to above 0.5%.
Methanol to oil molar ratio was varied for waste
cooking oil within the range of 3:1 to 9:1. The maximum
biodiesel yield for waste cooking oil was found at the
methanol to oil molar ratio of 6:1 in acid esterification. In
alkali transesterification, the maximum yield for waste
cooking oil was obtained at the methanol to oil molar
ratio of 9:1. The yield remains the moreover same with
further increase in the methanol to oil molar ratio. The

80

80

60

40

20

0
0

10

12

14

MeOH:Oil (Step 2)

Figure 2. Effect of molar ratio on biodiesel yield (Step 2) in


sulfuric acid process.
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Biodiesel Production from Waste Cooking Oil Using Sulfuric Acid and Microwave Irradiation Processes

in higher heat losses to the ambient. The energy required


by the conventional method is found to be around 11
times greater than that by the microwave method to
achieve same biodiesel yield for waste cooking oil. From
our previous study for camelina oil transesterification, it
was concluded that proper power dissipation control resulted in effective use of the microwave energy and further reduction in energy requirements [23].

Biodiesel Yield (%)

100

80

60

40

20

100
0
0

0.5

1.5

2.5

90

Figure 3. Effect of alkali catalyst amount on biodiesel yield


(Step 2) in sulfuric acid process.

pressure. The maximum yield was obtained at a temperature of 80C for waste cooking oil.

Biodiesel yield (% )

Alkali Conc. (wt%)

3.2. Microwave Catalytic Transesterification

Copyright 2012 SciRes.

70
KOH 1%
KOH 1.5%

60

KOH 2%
50

40
4

10

12

14

16

MeOH:Oil

Figure 4. Effect of methanol to oil molar ratio and catalyst


concentration (KOH) on biodiesel yield using microwave
method.
110
100

Bio diesel Yield (% )

The effect of methanol to oil molar ratio and catalyst


concentration (BaO and KOH) on waste biodiesel yield
using microwave method. Methanol-to-oil ratios of 6:1,
9:1, 12:1, and 15:1 were tested for both catalysts. In this
study, for homogeneous catalysts (KOH), a molar ratio
of 9:1 and 2% catalyst were found to be effective with
maximum biodiesel yield of 92% (Figure 4). For BaO, a
maximum biodiesel yield of 96% was obtained for 12:1
methanol to oil molar ratio and 2% catalyst concentration
(Figure 5). It was observed for homogeneous catalyst
that when the amount of methanol-to-oil molar ratio was
increased over 9:1, excess methanol started to interfere in
the separation of glycerin due to an increase in the solubility and resulted in lower biodiesel yield [27].
In combine effect of excess alcohol and KOH catalyst
leads to saponification resulting in lower biodiesel yield
and lower biodiesel quality. An advantage associated
with heterogeneous catalysts is that they can be recovered and reused several times. For homogeneous catalysts, the biodiesel separation and catalyst recovery from
reaction mixture can be laborious. The reactivity of BaO
catalyst was found to be quite different than KOH catalyst as it posses different catalytic activity, basicity, leaching tendency, and specific surface area, which influence
the transesterification of oil [28].
Energy requirements for the two heating methods (microwave and conventional) for waste cooking oil transesterification are presented in Table 1. It can be noted
that that 6 min were sufficient for microwave heating
while 105 min were required for conventional heating to
achieve comparable biodiesel yields. This large difference in reaction time can be attributed to the limitations
of conventional heating in which the energy is first utilized to increase the temperature of the reaction vessel
and the higher temperature of the reaction vessel results

80

90
80
70

BaO 1%
BaO 1.5%

60

BaO 2%

50
40
4

10

12

14

16

MeOH :Oil

Figure 5. Effect of methanol to oil molar ratio and catalyst


concentration (BaO) on biodiesel yield using microwave
method.
Table 1. Comparison of energy consumptions for biodiesel
production from waste cooking oil by two methods.

Energy dissipated (J/s)

Microwave
heating

Conventional
Catalyst
heating

800

500

Time of reaction (s)

360

6300

% Power emitted

100

100

Total energy required (kJ)

288

3150

Ratio

10.93

Biodiesel yield (%)

92

92

KOH

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Biodiesel Production from Waste Cooking Oil Using Sulfuric Acid and Microwave Irradiation Processes

The major benefits of microwave-assisted transesterification over conventional heating are: 1) Rate Enhancement: reaction times can be drastically reduced from hours
to minutes; 2) Increased yield: shorter reaction time minimizes unwanted side reactions; 3) Improved purity: less
by-products result in simplified purification.

3.3. Thermogravimetric Analysis of Waste


Cooking Oil and Biodiesel
Thermogravimetric analysis (TGA) is a technique for
characterizing thermal stability of a material (compound
or mixture) by measuring changes in its physicochemical
properties expressed as weight change as a function of
increasing temperature [29]. TGA is a simple, convenient,
and economical method for monitoring biodiesel production.
Figure 6 shows the TGA plot for waste cooking oil,
biodiesel and mixture of oil and biodiesel (50% - 50%).
TGA was performed on PerkinElmer Pyris 1 TGA instrument. The temperature range employed was 25C 600C. The mass of the waste cooking biodiesel starts to
decrease at approximately after 125C - 130C, and this
step was attributed to vaporization of biodiesel, and the
second step started to decrease at 232C, and it may be
due to some waste cooking oil that was not transesterified. TGA curve of waste cooking biodiesel did not show
any step afterwards, confirmed that the transesterification
reaction was complete. Similarly, evaporation of waste
cooking oil starts at approximately 325C. TGA curve for
waste cooking oil and biodiesel (50% - 50%) mixture
confirmed the combine effect of both samples at respective temperatures as discussed above. For mixture, it was

111

recorded that 0.9% loss of sample at 125C, 41.54% loss


at 232C and 98% loss at 460C. The percentage of biodiesel and waste cooking oil in a sample could be calculated from the TGA plot of the sample taking into account the first derivative of the weight change of the
sample mixture.
In addition, the mass loss recorded for biodiesel at
125C correlates the mass percentage of biodiesel present
in the sample. Likewise, the mass loss associated with
waste cooking oil (ca. 325C) correlates to the mass percentage of waste cooking oil in the sample. Because of
these temperatures vary by a relatively large value (approx
200C), this method should be quite effective in distinguishing biodiesel from waste cooking oil.

3.4. Fuel Properties of Methyl Esters


The fuel properties of biodiesel from waste cooking oil
(WCO) obtained from microwave process with testing
methods are given in Table 2. The viscosities of biodiesel from waste cooking oil was closer to that of viscosity of regular diesel i.e. 2.6 mm2/s. Hence, no hardware modifications are required for handling this fuel
(biodiesel) in the existing engine. The calorific value of
waste cooking oil ester was reported in the range of
45.08 - 45.24 MJ/kg. The cetane number was found to be
higher than ASTM standards for biodiesel. Higher cetane
number indicates good ignition quality of fuel. The pour
point of waste cooking biodiesel was found to be in between 4C - 1C. This pour point might give rise to low
running problems in cold season. This problem could be
overcome by the addition of suitable pour point depressants or by blending with diesel oil.

Figure 6. Overlay of thermogravimetric curves for waste cooking oil, biodiesel and mixture (50% - 50%) of waste cooking oil
and biodiesel.
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Biodiesel Production from Waste Cooking Oil Using Sulfuric Acid and Microwave Irradiation Processes
Table 2. Properties of methyl ester from waste cooking oil.
Waste
Cooking Oil

Waste cooking
methyl ester

Biodiesel standard
ASTM D 6751-09

Regular diesel

Testing method

0.92

0.87 - 0.88

0.86 - 0.90

0.85

ASTM D4052

Viscosity (mm /s) at 40C

28.8

2.25 - 3.10

1.9 - 6.0

2.6

ASTM D445

Calorific Value (MJ/kg)

44.44

45.08 - 45.24

Report

42

ASTM D240

Cetane Number

32.48

55.45 - 56.10

47 min.

46

ASTM D613

Pour Point (C)

12

4 to 1

Report

20

ASTM D97

Properties
Specific Gravity
2

4. Conclusion
The production of fuel quality biodiesel from low-cost
high FFA waste cooking oil was investigated. A two-step
transesterification process was used to convert the high
free fatty acid oil to its ester. Microwave-assisted transesterification of waste cooking oil using heterogeneous
and homogeneous was investigated for optimum reaction
conditions. The preliminary experimental study performed in this work has demonstrated that the microwave-heating method is energy-efficient and better than
the conventional heating method.

5. Acknowledgements
This project was partially supported by US Department
of Energy (DE-EE0003046) and US Air Force Research
Laboratory (FA8650-11-C-2127).

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